CN103651602B - Pesticide composition containing thymus mongolicus and common origanum extracts, and preparation method and application thereof - Google Patents
Pesticide composition containing thymus mongolicus and common origanum extracts, and preparation method and application thereof Download PDFInfo
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- CN103651602B CN103651602B CN201310739896.0A CN201310739896A CN103651602B CN 103651602 B CN103651602 B CN 103651602B CN 201310739896 A CN201310739896 A CN 201310739896A CN 103651602 B CN103651602 B CN 103651602B
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Abstract
The invention relates to a pesticide composition containing thymus mongolicus and common origanum extracts, and a preparation method and application thereof, and belongs to the field of pesticides. In order to solve technical problems, the invention provides the pesticide composition containing the thymus mongolicus and common origanum extracts, and the preparation method and application thereof. According to the pesticide composition containing the thymus mongolicus and common origanum extracts, active ingredients of the pesticide composition are extracted from 1 weight part of thymus mongolicus and 0.2 to 4 weight parts of common origanum. The pesticide composition containing the thymus mongolicus and common origanum extracts has an obvious effect of controlling rice blast and rust disease of crops, and is prepared from Chinese herbal medicines serving as raw materials, so the problem of pesticide residue is solved, environmental pollution is avoided, the pesticide effect concentration is low during use, and the cost is low.
Description
Technical field
The present invention relates to composition pesticide containing thyme and wild marjoram extract and its preparation method and application, belong to crop bactericide field.
Background technology
Thyme is the genus under Labiatae, comprises about 350 kinds of perennial fragrant herbaceous plant, the highest approximately 40 centimetres, is grown in Europe, north African and Asia.It is generally the narrow thin evergreen plant of stem.There is medical value, can bring mosquito repellent, pungent, tepor.Expel pathogenic wind from the body surface, promoting qi circulation and relieving pain, cough-relieving, step-down.For flu, cough, headache, toothache, indigestion, acute gastroenteritis, high blood pressure.
Wild marjoram has another name called only dysentery grass, Elsholtzia patrini garcke, south Sinkiang ziziphora herb, is Labiatae Origanum herbaceos perennial.Mainly be distributed in Mediterranean Region to the Central Asia, north African, North America and China most areas, hillside, roadside, shrubbery, meadow, the sylvan life of being born in height above sea level 500-3600m.Wild marjoram taste is pungent, cool in nature, nontoxic, and herb can be used as medicine, and has effect of urine detumescence of relieving superficies by cooling, regulating QI to expel dampness.Clinically treat the diseases such as yellow subcutaneous ulcer, heatstroke, heating, vomiting, acute gastroenteritis, stomachache for flu-prevention, its expelling cold and relieving exterior syndrome function is better than peppermint.
Rice blast is one of important disease of paddy rice, can cause the significantly underproduction, the underproduction 40%～50% when serious, and even No kernels or seeds are gathered, as in a year of scarcity.This disease all has generation in various places, wherein occur as many with leaf portion, joint portion, after generation, can cause the underproduction in various degree, especially panicle blast or joint pest occur early to weigh, and can cause dead ears so that total crop failure, mainly to use chemical agent to the control of rice blast now, as 40% Isoprothiolane, kasugarnycin, thiophanate-methyl, these medicaments can cause crops medicament residue, and can cause environmental pollution, long-term use, has produced resistance.
Rust is by the parasitogenic class plant disease of the rest fungus in fungi.Leaf, stem and the fruit of harm plant.Rest fungus generally only causes local infection, the position that is injured can produce the phlycten point of different colours or blister shape, cup-shaped, hair because of spore productive set, what have also can cause the symptoms such as tumour, tertia, Cong Zhi, Qu Zhi on limb, or causes fallen leaves, the burnt tip, undergrowth etc.When serious, sorus is intensive in flakes, plant is evaporated withered rapidly because moisture in body is a large amount of, rust distributes wide and harmfulness is large, be more common in cereal crop, leguminous plant and pears etc., mainly to use chemical agent to the control of rust now, the various medicaments such as amide-type medicament as sour in triazole type EBI agent, mebenils etc. such as triazolones, inorganic sulphur, these medicaments can cause crops medicament residue, and can cause serious environmental pollution.
To sum up, the medicament of finding the above-mentioned two Plants diseases of environmentally friendly control becomes a kind of new trend.
Summary of the invention
Technical problem to be solved by this invention is to provide containing composition pesticide of thyme and wild marjoram extract and its preparation method and application.
The present invention is containing the composition pesticide of thyme and wild marjoram extract, and its active component is extracted and formed by the crude drug of following weight portion: 1 part of thyme, 0.2～4 part of wild marjoram.
Wherein, preferably its active component is extracted and is formed by the crude drug of following weight portion: 1 part of thyme, 0.5～1.5 part of wild marjoram; More preferably its active component is extracted and is formed by the crude drug of following weight portion: 1 part of thyme, 0.8～1.2 part of wild marjoram; More preferably its active component is extracted and is formed by the crude drug of following weight portion: 1 part of thyme, 1 part of wild marjoram.
Extracting solvent used is organic solvent or water, preferred described organic solvent is methyl alcohol, ethanol, ethyl acetate, acetone, chloroform, more preferably described organic solvent is ethanol, the more preferably concentration >=60%v/v of ethanol, and more preferably described organic solvent is absolute ethyl alcohol.
Wherein, thyme and wild marjoram that the present invention adopts are Chinese herbal medicine, in order to improve the activity of the present invention containing the composition pesticide of thyme and wild marjoram extract, the thyme that thyme preferably dries in the shade, the leaf of Herba Origani that wild marjoram is preferably dried in the shade.
The present invention is containing the composition pesticide of thyme and wild marjoram extract, and after its active component is mixed by thyme and wild marjoram, common extraction forms; Or its active component extracts by thyme the thyme extract, the wild marjoram that obtain and extracts the wild marjoram extract obtaining and mix.
For cost-saving, improve the drug effect of agricultural chemicals, after its active component is preferably and is mixed by thyme and wild marjoram, common extraction forms.
Further, in order to improve containing thyme and the wild marjoram stability of the composition pesticide of extract altogether, in composition pesticide containing thyme and wild marjoram extract of the present invention, also comprise auxiliary agent, described auxiliary agent can adopt the usual auxiliaries in agricultural chemicals, as at least one in emulsifier, antifreeze, solvent, defoamer, dispersant, wetting agent and stabilizing agent.
Wherein, emulsifier can adopt at least one in non-ionic surface active agent and anion surfactant, described non-ionic surface active agent can be dibenzyl xenyl APEO, styryl phenyl APEO, styryl phenyl APEO, phenethyl phenyl polyoxyethylene one polyethenoxy ether, OPEO, alkylphenol polyoxyethylene sulfosuccinate, aliphatic acid polyethenoxy ether, fatty alcohol-polyoxyethylene ether, aliphatic amine polyoxyethylene ether, castor oil ethylene oxide adduct and derivative thereof, at least one in polyol fatty acid ester and ethylene oxide adduct etc. thereof, described anion surfactant is at least one in calcium dodecyl benzene sulfonate, alkylphenol polyoxyethylene phosphate, phenethyl phenol polyethenoxy ether phosphate etc., as emulsifier 500,601p, 602p etc., in addition, can also use commercially available emulsifier production.
Wherein, solvent can adopt at least one in water, ethanol, isopropyl alcohol, n-butanol, ethyl acetate, butyl acetate, methyl-sulfoxide, turpentine oil, solvent naphtha, 1-METHYLPYRROLIDONE, dimethyl formamide etc.
Wherein, antifreeze can be glycerine, propane diols, ethylene glycol, sodium chloride, calcium chloride, sorbierite etc.
Wherein, defoamer is silicone defoaming agent etc.;
Wherein, dispersant is at least one in lignosulfonates, PAA and propionamide copolymer, alkylnaphthalene sulfonate, polycarboxylic acid salt's condensation product, methyl sodiosul foaliphatate etc.
Wherein, wetting agent can be alkyl sulfate, alkylbenzenesulfonate, alkylnaphthalene sulfonate, aliphatic alcohol polyethenoxy base ether, alkylphenol-polyethenoxy base ether, sorbitan fatty acid ester etc.
Wherein, stabilizing agent can be 2-expoxy propane, butyl glycidyl ether, isopropyl alcohol, n-butanol, polyethylene glycol etc.
Composition pesticide containing thyme and wild marjoram extract of the present invention can be prepared into any one formulation that is applicable to agricultural use by the method for this area routine, for the ease of using, can make microemulsion, aqua or soluble concentrate.
Further, be preferably the soluble concentrate being formed by the component of following weight portion: thyme and wild marjoram extract, 1601,5 parts of dimethyl sulfoxide (DMSO)s of 500,15 parts of emulsifier of 3 parts of emulsifier and 37 parts of ethanol, wherein, thyme and wild marjoram extract be 40 weight portions crude drug extract form.
For the ease of storing and transport, can extract is concentrated, obtain concentrate, and then be prepared into various formulations, cycles of concentration can be adjusted voluntarily according to needs of production, as preferred version, thyme is prepared from by the following method with wild marjoram extract: crude drug is identical with crude drug weight through extracting and being concentrated into.
The present invention is made up of following steps containing the preparation method of the composition pesticide of thyme and wild marjoram extract:
A, extraction: take thyme and wild marjoram, mix, by solid-liquid ratio, 1:3～12g/ml adds solvent, in 60～95 DEG C of refluxing extraction, filter, and obtains filtrate, is extract, and wherein, described solvent is organic solvent or water;
B, preparation: extract is made to microemulsion, soluble concentrate or aqua.
Extract of the present invention adopts the filtrate obtaining through filtration after solvent extraction.
Wherein, thyme fruit and leaf of Herba Origani can adopt commercially available particle, also can adopt conventional method pulverizing thyme fruit and leaf of Herba Origani to obtain.In order to improve the effect of extraction, simultaneously cost-saving, thyme fruit and leaf of Herba Origani are crossed 60～100 mesh sieves, preferred mistake 80 mesh sieves.
Further, for cost-saving, simultaneously also in order to improve extraction efficiency, preferably in a step, solid-liquid ratio is 1:4～10g/ml, and more preferably in a step, solid-liquid ratio is 1:6g/ml.The thyme and the leaf of Herba Origani that are lg can add 3～12ml solvent extraction, preferably add 4～10ml solvent extraction, more preferably add 6ml solvent extraction.
Conventional organic solvent all can be used for the present invention, for cost-saving, improve dissolution rate, ensure extraction efficiency simultaneously, organic solvent is preferably methyl alcohol, ethanol, ethyl acetate, acetone, chloroform, more preferably described organic solvent is ethanol, the more preferably concentration >=60%v/v of ethanol, and more preferably described organic solvent is absolute ethyl alcohol.
Further, the temperature of preferred described backflow is 75～85 DEG C, and more preferably the temperature of described backflow is 80 DEG C.
Further, preferably reflow's cycle is twice, and the time that more preferably single refluxes is 1～3h, and the time that more preferably single refluxes is 2h; Merging filtrate, obtains extract.
Further, preferably in reflux course, stir, the rotating speed of stirring is 80～100 turn/min, and the rotating speed preferably stirring is 90 turn/min.
The present invention contains the composition pesticide of thyme and wild marjoram extract in the application preventing and treating in crop rice blast and rust.
Composition pesticide containing thyme and wild marjoram extract of the present invention, all has good preventive effect to rice blast and rust.
In actual agricultural production, in order to improve composition pesticide containing thyme and the wild marjoram extract control efficiency to rice blast and rust, the described composition pesticide containing thyme and wild marjoram extract is preferably applied to rice blast and rust their early stage; Composition pesticide containing thyme and wild marjoram extract of the present invention can be used by common method, sprays on plant leaf surface.
As preferred version, while using, be 10～100ppm containing the composition pesticide thin up of thyme and wild marjoram extract to the activity component concentration taking crude drug weighing scale by the present invention, get the composition pesticide making after 1g crude drug extracts, in the time using, be diluted with water to 10kg, its activity component concentration equals 100ppm; Further the agricultural chemicals after preferred dilution, taking the activity component concentration of crude drug weighing scale as 20～50ppm, sprays in plant blade face, and to occur water membrane on blade face, not lower of liquid is advisable; After being preferable over 5～7 days, carry out dispenser again, the preferred continuous administration of a season crop 2～3 times.
Its active component of composition pesticide containing thyme and wild marjoram extract of the present invention is by thyme extract and wild marjoram extract is composite forms, or its active component is extracted and is formed by thyme and wild marjoram mixing, its preventive effect is far away higher than the extract of single component, particularly thyme and wild marjoram are mixed to the composition pesticide that the rear jointly extract that extraction obtains is made, owing to having solubilising, hydrotropy effect between thyme and wild marjoram, the composition pesticide bactericidal effect of making after common extraction is more remarkable.
Compared with prior art, the composition pesticide containing thyme and wild marjoram extract of the present invention has the following advantages:
1, the present invention adopts herbaceous plant extract as active component containing the composition pesticide of thyme and wild marjoram extract, to crops drug residue free, can not be to environment.
2, the present invention extracts from thyme and leaf of Herba Origani containing the composition pesticide of thyme and wild marjoram extract, aspect control rice blast, rust, has outstanding effect, can play the effect for the treatment of after primary prevention, morbidity.
3, the present invention is wide containing the source of the plant material of the composition pesticide of thyme and wild marjoram extract, extracting method is simple, and valid density is low, with low cost while using.
4, the present invention has the effect of Synergistic containing the composition pesticide of thyme and wild marjoram extract, and the composition pesticide of making compared to independent thyme, wild marjoram extract is having more outstanding effect aspect control rice blast, rust.
Embodiment
Technical problem to be solved by this invention is to provide containing composition pesticide of thyme and wild marjoram extract and its preparation method and application.
The present invention is containing the composition pesticide of thyme and wild marjoram extract, and its active component is extracted and formed by the crude drug of following weight portion: 1 part of thyme, 0.2～4 part of wild marjoram.
Wherein, preferably its active component is extracted and is formed by the crude drug of following weight portion: 1 part of thyme, 0.5～1.5 part of wild marjoram; More preferably its active component is extracted and is formed by the crude drug of following weight portion: 1 part of thyme, 0.8～1.2 part of wild marjoram; More preferably its active component is extracted and is formed by the crude drug of following weight portion: 1 part of thyme, 1 part of wild marjoram.
Extracting solvent used is organic solvent or water, preferred described organic solvent is methyl alcohol, ethanol, ethyl acetate, acetone, chloroform, more preferably described organic solvent is ethanol, the more preferably concentration >=60%v/v of ethanol, and more preferably described organic solvent is absolute ethyl alcohol.
Wherein, thyme and wild marjoram that the present invention adopts are Chinese herbal medicine, in order to improve the activity of the present invention containing the composition pesticide of thyme and wild marjoram extract, the thyme that thyme preferably dries in the shade, the leaf of Herba Origani that wild marjoram is preferably dried in the shade.
The present invention is containing the composition pesticide of thyme and wild marjoram extract, and after its active component is mixed by thyme and wild marjoram, common extraction forms; Or its active component extracts by thyme the thyme extract, the wild marjoram that obtain and extracts the wild marjoram extract obtaining and mix.
For cost-saving, improve the drug effect of agricultural chemicals, after its active component is preferably and is mixed by thyme and wild marjoram, common extraction forms.
Further, in order to improve containing thyme and the wild marjoram stability of the composition pesticide of extract altogether, in composition pesticide containing thyme and wild marjoram extract of the present invention, also comprise auxiliary agent, described auxiliary agent can adopt the usual auxiliaries in agricultural chemicals, as at least one in emulsifier, antifreeze, solvent, defoamer, dispersant, wetting agent and stabilizing agent.
Wherein, emulsifier can adopt at least one in non-ionic surface active agent and anion surfactant, described non-ionic surface active agent can be dibenzyl xenyl APEO, styryl phenyl APEO, styryl phenyl APEO, phenethyl phenyl polyoxyethylene one polyethenoxy ether, OPEO, alkylphenol polyoxyethylene sulfosuccinate, aliphatic acid polyethenoxy ether, fatty alcohol-polyoxyethylene ether, aliphatic amine polyoxyethylene ether, castor oil ethylene oxide adduct and derivative thereof, at least one in polyol fatty acid ester and ethylene oxide adduct etc. thereof, described anion surfactant is at least one in calcium dodecyl benzene sulfonate, alkylphenol polyoxyethylene phosphate, phenethyl phenol polyethenoxy ether phosphate etc., as emulsifier 500,601p, 602p etc., in addition, can also use commercially available emulsifier production.
Wherein, solvent can adopt at least one in water, ethanol, isopropyl alcohol, n-butanol, ethyl acetate, butyl acetate, methyl-sulfoxide, turpentine oil, solvent naphtha, 1-METHYLPYRROLIDONE, dimethyl formamide etc.
Wherein, antifreeze can be glycerine, propane diols, ethylene glycol, sodium chloride, calcium chloride, sorbierite etc.
Wherein, defoamer is silicone defoaming agent etc.;
Wherein, dispersant is at least one in lignosulfonates, PAA and propionamide copolymer, alkylnaphthalene sulfonate, polycarboxylic acid salt's condensation product, methyl sodiosul foaliphatate etc.
Wherein, wetting agent can be alkyl sulfate, alkylbenzenesulfonate, alkylnaphthalene sulfonate, aliphatic alcohol polyethenoxy base ether, alkylphenol-polyethenoxy base ether, sorbitan fatty acid ester etc.
Wherein, stabilizing agent can be 2-expoxy propane, butyl glycidyl ether, isopropyl alcohol, n-butanol, polyethylene glycol etc.
Composition pesticide containing thyme and wild marjoram extract of the present invention can be prepared into any one formulation that is applicable to agricultural use by the method for this area routine, for the ease of using, can make microemulsion, aqua or soluble concentrate.
Further, be preferably the soluble concentrate being formed by the component of following weight portion: thyme and wild marjoram extract, 1601,5 parts of dimethyl sulfoxide (DMSO)s of 500,15 parts of emulsifier of 3 parts of emulsifier and 37 parts of ethanol, wherein, thyme and wild marjoram extract be 40 weight portions crude drug extract form.
For the ease of storing and transport, can extract is concentrated, obtain concentrate, and then be prepared into various formulations, cycles of concentration can be adjusted voluntarily according to needs of production, as preferred version, thyme is prepared from by the following method with wild marjoram extract: crude drug is identical with crude drug weight through extracting and being concentrated into.
The present invention is made up of following steps containing the preparation method of the composition pesticide of thyme and wild marjoram extract:
A, extraction: take thyme and wild marjoram, mix, by solid-liquid ratio, 1:3～12g/ml adds solvent, in 60～95 DEG C of refluxing extraction, filter, and obtains filtrate, is extract, and wherein, described solvent is organic solvent or water;
B, preparation: extract is made to microemulsion, soluble concentrate or aqua.
Extract of the present invention adopts the filtrate obtaining through filtration after solvent extraction.
Wherein, thyme fruit and leaf of Herba Origani can adopt commercially available particle, also can adopt conventional method pulverizing thyme fruit and leaf of Herba Origani to obtain.In order to improve the effect of extraction, simultaneously cost-saving, thyme fruit and leaf of Herba Origani are crossed 60～100 mesh sieves, preferred mistake 80 mesh sieves.
Further, for cost-saving, simultaneously also in order to improve extraction efficiency, preferably in a step, solid-liquid ratio is 1:4～10g/ml, and more preferably in a step, solid-liquid ratio is 1:6g/ml.The thyme and the leaf of Herba Origani that are lg can add 3～12ml solvent extraction, preferably add 4～10ml solvent extraction, more preferably add 6ml solvent extraction.
Conventional organic solvent all can be used for the present invention, for cost-saving, improve dissolution rate, ensure extraction efficiency simultaneously, organic solvent is preferably methyl alcohol, ethanol, ethyl acetate, acetone, chloroform, more preferably described organic solvent is ethanol, the more preferably concentration >=60%v/v of ethanol, and more preferably described organic solvent is absolute ethyl alcohol.
Further, the temperature of preferred described backflow is 75～85 DEG C, and more preferably the temperature of described backflow is 80 DEG C.
Further, preferably reflow's cycle is twice, and the time that more preferably single refluxes is 1～3h, and the time that more preferably single refluxes is 2h; Merging filtrate, obtains extract.
Further, preferably in reflux course, stir, the rotating speed of stirring is 80～100 turn/min, and the rotating speed preferably stirring is 90 turn/min.
The present invention contains the composition pesticide of thyme and wild marjoram extract in the application preventing and treating in crop rice blast and rust.
Composition pesticide containing thyme and wild marjoram extract of the present invention, all has good preventive effect to rice blast and rust.
In actual agricultural production, in order to improve composition pesticide containing thyme and the wild marjoram extract control efficiency to rice blast and rust, the described composition pesticide containing thyme and wild marjoram extract is preferably applied to rice blast and rust their early stage; Composition pesticide containing thyme and wild marjoram extract of the present invention can be used by common method, sprays on plant leaf surface.
As preferred version, while using, be 10～100ppm containing the composition pesticide thin up of thyme and wild marjoram extract to the activity component concentration taking crude drug weighing scale by the present invention, get the composition pesticide making after 1g crude drug extracts, in the time using, be diluted with water to 10kg, its activity component concentration equals 100ppm; Further the agricultural chemicals after preferred dilution, taking the activity component concentration of crude drug weighing scale as 20～50ppm, sprays in plant blade face, and to occur water membrane on blade face, not lower of liquid is advisable; After being preferable over 5～7 days, carry out dispenser again, the preferred continuous administration of a season crop 2～3 times.
Its active component of composition pesticide containing thyme and wild marjoram extract of the present invention is by thyme extract and wild marjoram extract is composite forms, or its active component is extracted and is formed by thyme and wild marjoram mixing, its preventive effect is far away higher than the extract of single component, particularly thyme and wild marjoram are mixed to the composition pesticide that the rear jointly extract that extraction obtains is made, owing to having solubilising, hydrotropy effect between thyme and wild marjoram, the composition pesticide bactericidal effect of making after common extraction is more remarkable.
Below in conjunction with embodiment, the specific embodiment of the present invention is further described, does not therefore limit the present invention among described scope of embodiments.
Embodiment 1 is containing the preparation of the composition pesticide of thyme and wild marjoram extract
A, extraction: get thyme fruit after drying, leaf of Herba Origani after drying in the shade, mix, pulverize, cross 80 mesh sieves, add wherein solvent, stir evenly, heat up, turn on agitator, it is 90 turn/min that rotating speed is set, refluxing extraction, extraction completes, and filters, collects filtrate;
In filter residue, add solvent, stir evenly, heat up, turn on agitator, rotating speed is 90 turn/min, refluxing extraction is filtered, and collects filtrate;
The filtrate of twice collection is merged, filtrate is concentrated to the weight of crude drug, obtain thyme and wild marjoram extract bn-01～bn-07, refrigeration, wherein, parameter when bn-01～bn-07 extract extracts is in table 1.
B, preparation: auxiliary agent add table 2 in extract bn-01～bn-07 in, stir, must be containing the composition pesticide BN-01～BN-07 of thyme and wild marjoram extract, wherein, containing the formula of the composition pesticide BN-01～BN-07 of thyme and wild marjoram extract in table 2.
The preparation technology parameter of table 1 thyme and wild marjoram extract
Table 2 is containing the formula of the composition pesticide of thyme and wild marjoram extract
Embodiment 2 is containing the preparation of the composition pesticide of thyme and wild marjoram extract
A, extraction: the thyme fruit of getting after drying is pulverized, and crosses 80 mesh sieves, adds wherein solvent, stirs evenly, heat up, turn on agitator, and it is 90 turn/min that rotating speed is set, refluxing extraction, extraction completes, and filters, collects filtrate; According to the method described above filter residue is extracted again, merge the filtrate that extracted twice obtains, by filtrate simmer down to crude drug weight, obtain thyme extract d1-01～d1-03, wherein, each parameter is in table 3;
Get the leaf of Herba Origani after drying in the shade, cross 80 mesh sieves, add wherein solvent, stir evenly, heat up, turn on agitator, it is 90 turn/min that rotating speed is set, refluxing extraction, extraction completes, and filters, collects filtrate; According to the method described above filter residue is extracted again, merge the filtrate that extracted twice obtains, by filtrate simmer down to crude drug weight, obtain wild marjoram extract d2-01～d2-03, wherein, each parameter is in table 4;
B, preparation: take thyme extract, wild marjoram extract and auxiliary agent, stirring and evenly mixing, obtains the composition pesticide BN-08～BN-12 containing thyme and wild marjoram extract, and wherein, each parameter is in table 5.
The refluxing extraction parameter of table 3 thyme extract
The refluxing extraction parameter of table 4 wild marjoram extract
Table 5 is containing the formula of the composition pesticide of thyme and wild marjoram extract
The preparation of comparative example 1 thyme extract soluble concentrate
Get the d1-01 in 400g embodiment 2, add 30g emulsifier 500,150g emulsifier 1601, dimethyl sulfoxide (DMSO) 50g, ethanol 370g, stirring and evenly mixing, obtains thyme extract soluble concentrate, is designated as D1.
The preparation of comparative example 2 wild marjoram extract soluble concentrates
Get the d2-01 in 400g embodiment 2, add 30g emulsifier 500,150g emulsifier 1601, dimethyl sulfoxide (DMSO) 50g, ethanol 370g, stirring and evenly mixing, obtains wild marjoram extract soluble concentrate, is designated as D2.
In above-described embodiment, comparative example, thyme and wild marjoram are purchased from Anguo City Zhong Tian prepared slices of Chinese crude drugs Co., Ltd.
Test of pesticide effectiveness part:
For clearly putting into field efficacy situation containing the composition pesticide of thyme and wild marjoram extract, inventor has carried out field control effectiveness test to this medicament.
The control rice blast test of pesticide effectiveness---paddy rice
For studying thing: paddy rice.
Reagent agent: the product in embodiment: BN-01～BN-14; Single dose contrast in comparative example: D1 and D2; Chemical agent contrast: Fujione (B1) (Longdeng Chemical Co Ltd, Jiangsu's production); Clear water contrast (CK).
14 medicaments of this test, 2 single dose contrasts, 1 contrast medicament, 1 blank, repeats Gong54Ge community for three times.Minizone and surrounding all leave isolation strip, community area 20m
2, randomized arrangement is respectively processed in community.
It is 50ppm that reagent agent is diluted to activity component concentration, and the reagent agent of getting after dilution sprays application to plant blade face, and to occur water membrane on blade face, not lower of liquid is advisable.
Spray three times, in the time that rice blast is fallen ill, start to spray, spray for the first time and interval for the second time 9 days, spray for the second time and spray for the third time interval 9 days.Carry out 2 investigation, spray for the first time front investigation once, spray for the third time investigation in rear ten days once.Four of investigation standard Wei Ge communities end points and central point thereof be totally five points, and each point is chosen 50 fringe fruit ears, chooses altogether 250 fringe fruit ears and investigate.
Data processing after investigation:
The computational methods of disease index: disease index=∑ (sick spike numbers at different levels × numerical value that represents at different levels)/(total sample number × highest typical value) × 100.
Preventive effect (%)=[before the dispenser of 1-(check plot, after the dispenser of refer to × treatment region of disease, disease refers to)/(after the dispenser of check plot, before the dispenser of sick index × treatment region, disease refers to)] × 100%.
Rice blast severity Scaling standard is in table 6:
Table 6 rice blast severity Scaling standard
| Grade | Symptom |
| 0 grade | All anosis |
| 1 grade | Every fringe loses below 5% |
| 3 grades | Every fringe loss 6%-20% |
| 5 grades | Every fringe loss 21%-50% |
| 7 grades | Every fringe loss 51%-70% |
| 9 grades | Every fringe loss 71%-100% |
Survey data is 3 mean values that repeat.
Before spraying for the first time, investigate, survey data is in table 7:
The result that table 7 is investigated before spraying for the first time
For the second time after investigation the parameter that obtains in table 8:
The parameter that table 8 obtains after investigating for the second time
As shown in Table 8, the present invention is containing the composition pesticide energy effectively preventing rice blast of thyme and wild marjoram extract, preventive effect reaches more than 56.51%, have better effect compared to independent thyme extract preventive effect 16.39%, wild marjoram extract preventive effect 15.65%, the present invention has the effect of Synergistic containing the composition pesticide of thyme and wild marjoram extract.
The control rust test of pesticide effectiveness---cowpea
For studying thing: cowpea.
Reagent agent: the product in embodiment: BN-01～BN-14; Single dose contrast in comparative example: D1 and D2; Chemical agent contrast: take enemy steady (B1), take enemy to be surely purchased from Beyer Co., Ltd; Clear water contrast (CK).
14 medicaments of this test, 2 single dose contrasts, 1 contrast medicament, 1 blank, repeats Gong54Ge community for three times.Minizone and surrounding all leave isolation strip, community area 20m
2, randomized arrangement is respectively processed in community.
It is 50ppm that reagent agent is diluted to activity component concentration, and the reagent agent of getting after dilution sprays application to plant blade face, and to occur water membrane on blade face, not lower of liquid is advisable.
Spray three times, in the time that asparagus bean rust is fallen ill, start to spray, spray for the first time and interval for the second time 7 days, spray for the second time and spray for the third time interval 7 days.Carry out 2 investigation, spray for the first time front investigation once, spray for the third time investigation in latter 16 days once.Four of investigation standard Wei Ge communities end points and central point thereof be totally five points, and each point is chosen 20 leaves, chooses altogether 100 leaves and investigate.Data processing after investigation:
Disease index=∑ (the sick numbers of sheets at different levels × numerical value that represents at different levels)/(total sample number × highest typical value) × 100.
Preventive effect (%)=[before the dispenser of the blank group of 1-(, after the dispenser of refer to × treatment region of disease, disease refers to)/(after the dispenser of blank group, before the dispenser of sick index × treatment region, disease refers to)] × 100%.
Asparagus bean rust severity Scaling standard is in table 9.
Table 9 asparagus bean rust severity Scaling standard
| Grade | Symptom |
| 0 grade | All anosis |
| 1 grade | Lesion area accounts for leaf area below 5% |
| 3 grades | Lesion area accounts for leaf area 6%-25% |
| 5 grades | Lesion area accounts for leaf area 26%-50% |
| 7 grades | Lesion area accounts for leaf area 51%-75% |
| 9 grades | Lesion area is more than 76% |
Survey data is 3 mean values that repeat.
Before spraying for the first time, investigate, survey data is in table 10:
The result that table 10 is investigated before spraying for the first time
For the second time after investigation the parameter that obtains in table 11:
The parameter that table 11 obtains after investigating for the second time
As shown in Table 11, the present invention is containing the composition pesticide energy effectively preventing rust of thyme and wild marjoram extract, preventive effect reaches more than 56.81%, have better effect compared to independent thyme extract preventive effect 18.40%, wild marjoram extract preventive effect 15.05%, the present invention has the effect of Synergistic containing the composition pesticide of thyme and wild marjoram extract.
Claims (15)
1. contain the composition pesticide of thyme and wild marjoram extract, it is characterized in that: it is soluble concentrate, described soluble concentrate is made up of the component of following weight portion: thyme and wild marjoram extract, 1601,5 parts of dimethyl sulfoxide (DMSO)s of 500,15 parts of emulsifier of 3 parts of emulsifier and 37 parts of ethanol, wherein, thyme and wild marjoram extract be 40 weight portions crude drug extract form; Thyme is prepared from by the following method with wild marjoram extract: crude drug is identical with crude drug weight through extracting and being concentrated into, and in crude drug, the weight proportion of thyme and wild marjoram is: thyme: wild marjoram=1:0.2～4.
2. the composition pesticide containing thyme and wild marjoram extract according to claim 1, is characterized in that: in crude drug, the weight proportion of thyme and wild marjoram is: thyme: wild marjoram=1:0.5～1.5.
3. the composition pesticide containing thyme and wild marjoram extract according to claim 2, is characterized in that: in crude drug, the weight proportion of thyme and wild marjoram is: thyme: wild marjoram=1:0.8～1.2.
4. the composition pesticide containing thyme and wild marjoram extract according to claim 3, is characterized in that: in crude drug, the weight proportion of thyme and wild marjoram is: thyme: wild marjoram=1:1.
5. according to the composition pesticide containing thyme and wild marjoram extract described in claim 1～4 any one, it is characterized in that: after thyme and wild marjoram extract are mixed by thyme and wild marjoram, common extraction forms; Or thyme and wild marjoram extract extract by thyme the thyme extract, the wild marjoram that obtain and extract the wild marjoram extract obtaining and mix.
6. the preparation method of the composition pesticide containing thyme and wild marjoram extract described in claim 1～4 any one, is characterized in that: be made up of following steps:
A, extraction: take thyme and wild marjoram, mix, by solid-liquid ratio, 1:3～12g/ml adds solvent, in 60～95 DEG C of refluxing extraction, filter, and obtains filtrate, i.e. extract, and wherein, described solvent is organic solvent or water;
B, preparation: extract is made to soluble concentrate.
7. the preparation method of the composition pesticide containing thyme and wild marjoram extract according to claim 6, is characterized in that:
In described a step, thyme and wild marjoram cross 60～100 mesh sieves; Described solid-liquid ratio is 1:4～10 g/ml; Described organic solvent is methyl alcohol, ethanol, ethyl acetate, acetone or chloroform, and the temperature of described backflow is 75～85 DEG C; The time of described backflow is 1～3h; Reflow's cycle is twice, and merging filtrate, obtains extract.
8. the preparation method of the composition pesticide containing thyme and wild marjoram extract according to claim 7, is characterized in that:
In described a step, thyme and wild marjoram 80 mesh sieves; Described solid-liquid ratio is 1:6 g/ml; Described organic solvent is ethanol, the concentration >=60%v/v of ethanol; The temperature of described backflow is 80 DEG C; The time of described backflow is 2h.
9. the preparation method of the composition pesticide containing thyme and wild marjoram extract according to claim 8, is characterized in that:
In described a step, described organic solvent is absolute ethyl alcohol.
10. the application of the composition pesticide containing thyme and wild marjoram extract described in claim 1～4 any one in control crop rice blast and rust.
11. composition pesticides containing thyme and wild marjoram extract according to claim 10, in the application of control crop rice blast and rust, is characterized in that: when application, thin up is 10～100ppm to the concentration of the active component taking crude drug weighing scale.
12. composition pesticides containing thyme and wild marjoram extract according to claim 11, in the application of control crop rice blast and rust, is characterized in that: thin up is 20～50ppm to the concentration taking crude drug extract.
The application of the composition pesticide containing thyme and wild marjoram extract that preparation method described in 13. claim 6-9 any one makes in control crop rice blast and rust.
The composition pesticide containing thyme and wild marjoram extract that 14. preparation methods according to claim 13 make is in the application of control crop rice blast and rust, it is characterized in that: when application, thin up is 10～100ppm to the concentration of the active component taking crude drug weighing scale.
The composition pesticide containing thyme and wild marjoram extract that 15. preparation methods according to claim 14 make, in the application of control crop rice blast and rust, is characterized in that: thin up is 20～50ppm to the concentration taking crude drug extract.
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| CN107488059A (en) * | 2017-07-28 | 2017-12-19 | 惠州市锦恒工业模具设计合伙企业(普通合伙) | A kind of Bactericide fertilizer based on turmeric root tuber extract |
| CN109497100B (en) * | 2019-01-11 | 2021-08-10 | 成都新朝阳作物科学股份有限公司 | Pesticide composition containing oregano and rosemary extracts and preparation method and application thereof |
| CN109673687A (en) * | 2019-01-23 | 2019-04-26 | 成都新朝阳作物科学有限公司 | Composition pesticide of the Bulbus Allii Cepae extract containing wild marjoram and its preparation method and application |
| CN110506760A (en) * | 2019-08-14 | 2019-11-29 | 山东劲脉植物细胞信息技术有限公司 | A kind of plant biological composition, preparation and its method of administration |
| CN112219865A (en) * | 2020-10-12 | 2021-01-15 | 兰州大学 | Application of oregano essential oil in preventing and treating plant-derived germs |
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